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p-Toluenesulphonyl cyanide → 8-Oxospiro[4.5]decane-7-carbonitrile

HRID 1852476
ノート
印刷プレビュー

反応式

HRID 1852476 の反応式
[Li+].C[CH:3]([N-:5]C(C)C)C.[CH2:9]1[C:13]2([CH2:18][CH2:17][C:16](=[O:19])[CH2:15][CH2:14]2)[CH2:12][CH2:11][CH2:10]1.S(C#N)(C1C=CC(C)=CC=1)(=O)=O>C1COCC1>[O:19]=[C:16]1[CH2:17][CH2:18][C:13]2([CH2:9][CH2:10][CH2:11][CH2:12]2)[CH2:14][CH:15]1[C:3]#[N:5]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 87946p-Toluenesulphonyl cyanideHCID 2724682Lithium diisopropylamideHCID 14626805Spiro(4.5)decan-8-one

生成物 1

HCID 867310138-Oxospiro[4.5]decane-7-carbonitrile

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
-78 °C

実験手順

LDA (1.83 mL, 3.66 mmol, 2.0 M in hexanes) was combined with THF (3.2 mL) and cooled to −78° C. To this mixture was added a solution of spiro[4.5]decan-8-one (0.50 g, 3.3 mmol) in THF (3.2 mL). The resulting mixture was stirred at −78° C. for 20 mins then taken up in a syringe and added to a mixture of tosyl cyanide (0.59 g, 3.3 mmol) in THF (3.2 mL) at −78° C. The reaction mixture was allowed to stir at −78° C. for 45 mins then quenched with 0.5M NaOH and extracted with EtOAc (2×). The combined organic extracts were washed with 1N aqueous HCl, brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo. The crude residue was purified by MPLC on silica gel (using a gradient elution of 0-50% EtOAc/hexanes). Desired fractions were identified, combined and concentrated in vacuo to afford the title compound. The residue was carried forward without further purification.

後処理

  1. customthen taken up in a syringe
  2. stirringto stir at −78° C. for 45 mins
  3. customthen quenched with 0.5M NaOH
  4. extractionextracted with EtOAc (2×)
  5. washThe combined organic extracts were washed with 1N aqueous HCl, brine
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude residue was purified by MPLC on silica gel (
  10. washa gradient elution of 0-50% EtOAc/hexanes)
  11. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b2522bd082f24ec79461117fe80458d7
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08962608B2

反応ノート

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